Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
  • C08J5/18—Manufacture of films or sheets
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
  • C08B11/00—Preparation of cellulose ethers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B25—HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
  • B25J—MANIPULATORS; CHAMBERS PROVIDED WITH MANIPULATION DEVICES
  • B25J5/00—Manipulators mounted on wheels or on carriages
  • B25J5/007—Manipulators mounted on wheels or on carriages mounted on wheels
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
  • D01D5/00—Formation of filaments, threads, or the like
  • D01D5/06—Wet spinning methods
• • D—TEXTILES; PAPER
  • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
  • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
  • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
  • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
  • C08J2301/02—Cellulose; Modified cellulose

Definitions

• the present invention relates to a method for producing a cellulosic shaped body, in which a cellulosic amine oxide solution is pressed through a nozzle or a gap, then passed through an air gap and finally coagulated in a precipitation bath.
• fibers with good performance properties can only be obtained from high polymers if a "fiber structure" can be achieved (Ullmann, 5th edition vol. A10, 456).
• a fiber structure can be achieved (Ullmann, 5th edition vol. A10, 456).
• melt spinning the fibers are stretched in the warm, plastic state while the molecules are still mobile, and dissolved polymers can be spun dry or wet.
• dry spinning drawing takes place while the solvent escapes or evaporates; the threads extruded into a coagulation bath are drawn during the coagulation.
• Methods of this type are known and are well described. In all these cases, it is important that the transition from the liquid state (regardless of whether melt or solution) to the solid state takes place in such a way that the polymer chains or chain packages (i.e. fibrids, fibrils, etc.) are also oriented during thread formation can be.
• EP-A-295 672 describes the production of aramid fibers, which are introduced, stretched and introduced into a non-coagulating medium via an air gap are then coagulated.
• DD-PS 218 121 deals with the spinning of cellulose in amine oxides via an air gap, measures being taken to prevent sticking.
• U.S. Patent 3,414,645 also describes the preparation of aromatic polyamides from solutions in a dry-wet spinning process.
• a disadvantage of this method is the lack of flexibility to be able to change the properties of the molded body.
• a minimal spin-draw ratio is required to obtain the appropriate textile data. With very little warping, only extremely modest textile fiber properties can be achieved, that is to say, for example, that fiber production results in extremely low working capacity (this is the product of fiber strength and fiber elongation).
• Another disadvantage is that the effect of the so-called withdrawal / exit velocity resonance (cf. Navard, Haudin, "Spinning of a Cellulose N-Methylmorpholine-N-oxide solution", Polymer Process Engineering, 3 (3), 291 (1985)) , which leads to irregular fiber diameters, the greater the larger the spin-draw ratio.
• the shape can practically only take place in the air gap. Subsequent shaping is very difficult. This naturally limits the range of possible products. A subsequent influencing of the product properties would be desirable, as a result of which this process is given considerable flexibility.
• the object of the present invention is to eliminate these disadvantages.
• This object is achieved according to the invention by a method of the type mentioned at the outset in that the ratio of take-off speed to hole exit speed is at most 1 and that the shaped body is stretched or deep-drawn after coagulation.
• the take-off speed is therefore less (or at most equal) to the hole exit speed of the spinning mass, so that no stretching can occur; this keeps the cellulose in a relatively unoriented state until it coagulates in the precipitation bath.
• This is advantageous because the lower the orientation before or during coagulation, the greater the possibility of influencing the properties afterwards. Due to the poor orientation, the coagulated (precipitated) cellulose has an elasticity that is almost reminiscent of rubber. According to the invention, this cellulose can now be stretched or deep-drawn to obtain the desired properties; This ensures the desired flexibility.
• Another advantage is that due to the no longer existing stretching of the air gap can be made almost as short, so that even if the spinnerets have a very high hole density, there is no danger that adjacent threads stick together. Since productivity can be significantly increased in large-scale production by increasing the hole density, this is also an essential advantage of the present invention.
• EXAMPLE 1 Production of a fiber with a ratio of take-off speed to hole exit speed of less than 1 (comparative test)
• a 13% cellulosic NMMO solution (pulp of the Viskokraft type from ICP, 10% water, 77% NMMO, 0.1% oxalic acid as stabilizer) was pressed through a nozzle with 100 holes (hole diameter 130 ⁇ m each). The output was 16.5 g / min; the resulting ejection speed was 10.35 m / min.
• the 100 threads were passed through an 8 mm long air gap and then at a speed of 6 m / min through a 15 cm long spinning bath (temperature: 2 ° C., NMMO concentration: 5%). The ratio of withdrawal speed to exit speed was therefore 0.58.
• the resulting fiber had a tenacity of 11.8 cN / tex with an elongation of 77.5%.
• the stretch value is extremely high; this proves that the cellulose is in a relatively disordered state.
• the fiber was again passed as in Example 1 through a spinning bath at 6 m / min (take-off / exit speed: 0.58) and then through an 80 cm long drawing bath with water (temperature: 77 ° C.).
• the second godet was operated at two different speeds v.
• the fibers obtained had the following properties: vm / min Draw% Titre dtex Firmness cond. cN / tex Elongation cond. % 14 133 32.4 19.7 17.5 21 250 10.3 22.3 9.2
• EXAMPLE 4 Production of a fiber with a ratio of take-off speed to hole exit speed of greater than 1 (comparative test)
• a 13% cellulosic NMMO solution (pulp of the Visokraft type from ICP, 10% water, 77% NMMO, 0.1% oxalic acid as stabilizer) was pressed through a nozzle with 100 holes (hole diameter 70 ⁇ m in each case).
• the delivery rate was 5.1 g / min, which corresponds to an exit speed of 11.1 m / min.
• the take-off speed of the first godet was 33.3 m / min. H. the ratio of take-off to exit speed was 3.0.
• the threads were passed through a spinning bath, the temperature of which was 33 ° C. and the NMMO concentration was 10%.
• the subsequent draw bath had a temperature of 79 ° C and an NMMO concentration of 9%.
• the second godet after the drawing bath had a take-off speed of 46.9 m / min. H. the draw was 41%.
• a 9% cellulosic NMMO solution (pulp of the type Buckeye V5 from Procter & Gamble, 12% water, 79% NMMO, 0.1% oxalic acid as stabilizer) was passed through a slot nozzle (gap: 50 ⁇ m; length: 30 mm ) pressed. The output was 21.3 g / min, which corresponds to an exit speed of 11.7 m / min.
• the extruded solution was drawn off through a 7 mm long air gap and then through a 15 cm long spinning bath (temperature: 24 ° C; NMMO concentration: 20%) using a first godet at a speed of 6 m / min. The ratio of withdrawal speed to exit speed was therefore 0.51.
• the film was passed through an 80 cm stretching bath (temperature: 90 ° C; concentration: 20%) and stretched with a second godet (speed: 11 m / min). The draw was therefore 83%.
• the properties of the washed and dried film were: thickness: 10 ⁇ m; Strength: 200 N / mm 2 ; Elongation: 6.5%.
• a film was produced as in Example 5, but not stretched, i.e. after the first godet, the film was removed. In the undrawn state, it was deep-drawn 3 mm with a glass rod, washed and dried, resulting in a stable molded body.

Landscapes

• Engineering & Computer Science (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Polymers & Plastics (AREA)
• Textile Engineering (AREA)
• Health & Medical Sciences (AREA)
• Manufacturing & Machinery (AREA)
• Medicinal Chemistry (AREA)
• Materials Engineering (AREA)
• Organic Chemistry (AREA)
• Mechanical Engineering (AREA)
• Robotics (AREA)
• General Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Biochemistry (AREA)
• Artificial Filaments (AREA)
• Polysaccharides And Polysaccharide Derivatives (AREA)
• Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
• Manufacture Of Macromolecular Shaped Articles (AREA)

Applications Claiming Priority (2)

Publications (3)

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ID=3479697

Family Applications (1)

Country Status (28)

Cited By (2)

Families Citing this family (20)

Family Cites Families (5)

• 1991
  • 1991-01-09 AT AT0003191A patent/AT395862B/de not_active IP Right Cessation
  • 1991-12-17 AU AU89798/91A patent/AU648618B2/en not_active Ceased
  • 1991-12-19 MA MA22657A patent/MA22373A1/fr unknown
  • 1991-12-23 YU YU197691A patent/YU47786B/sh unknown
  • 1991-12-27 ZA ZA9110159A patent/ZA9110159B/xx unknown
• 1992
  • 1992-01-06 RO RO149066A patent/RO107703B1/ro unknown
  • 1992-01-06 ZW ZW1/92A patent/ZW192A1/xx unknown
  • 1992-01-06 KR KR1019920000040A patent/KR100210294B1/ko not_active IP Right Cessation
  • 1992-01-06 BG BG095726A patent/BG60110B2/bg unknown
  • 1992-01-08 NO NO920105A patent/NO303738B1/no not_active IP Right Cessation
  • 1992-01-08 IE IE005392A patent/IE920053A1/en not_active IP Right Cessation
  • 1992-01-08 RU SU925010549A patent/RU2061115C1/ru not_active IP Right Cessation
  • 1992-01-08 JP JP4001348A patent/JP3072442B2/ja not_active Expired - Lifetime
  • 1992-01-08 PT PT99990A patent/PT99990A/pt not_active Application Discontinuation
  • 1992-01-08 FI FI920071A patent/FI102391B/fi not_active IP Right Cessation
  • 1992-01-08 HU HU9200066A patent/HU212701B/hu not_active IP Right Cessation
  • 1992-01-08 PL PL92293116A patent/PL169424B1/pl unknown
  • 1992-01-08 CA CA002059042A patent/CA2059042C/en not_active Expired - Fee Related
  • 1992-01-08 BR BR929200035A patent/BR9200035A/pt not_active IP Right Cessation
  • 1992-01-08 CZ CS9245A patent/CZ282935B6/cs unknown
  • 1992-01-08 SK SK45-92A patent/SK280035B6/sk unknown
  • 1992-01-09 DE DE59208903T patent/DE59208903D1/de not_active Expired - Lifetime
  • 1992-01-09 TR TR92/0017A patent/TR25874A/xx unknown
  • 1992-01-09 IL IL100619A patent/IL100619A0/xx unknown
  • 1992-01-09 EP EP92890003A patent/EP0494851B1/de not_active Expired - Lifetime
  • 1992-01-09 ES ES92890003T patent/ES2109333T3/es not_active Expired - Lifetime
  • 1992-01-09 MX MX9200098A patent/MX9200098A/es not_active IP Right Cessation
• 1997
  • 1997-12-10 GR GR970403284T patent/GR3025632T3/el unknown

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